CN112125327B - Preparation process of active zinc oxide - Google Patents
Preparation process of active zinc oxide Download PDFInfo
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- CN112125327B CN112125327B CN202011008403.2A CN202011008403A CN112125327B CN 112125327 B CN112125327 B CN 112125327B CN 202011008403 A CN202011008403 A CN 202011008403A CN 112125327 B CN112125327 B CN 112125327B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention belongs to the field of active zinc oxide preparation, and particularly discloses a preparation process of active zinc oxide, which comprises the steps of (1) collecting zinc-containing smoke dust, (2) microwave heating, (3) basic zinc carbonate pretreatment, (4) drying and (5) calcining; the invention promotes the generation of the intermediate small-particle-size basic zinc carbonate by the combined control of microwaves and ultrasound, and finally the prepared zinc oxide has small particle size, high purity, good uniformity and large specific surface area.
Description
Technical Field
The invention belongs to the field of preparation of active zinc oxide, and particularly discloses a preparation process of active zinc oxide.
Background
The active zinc oxide is an important inorganic fine chemical product, is mainly used as reinforcing agent and active agent of rubber and cable, can obviously raise strength and wear resistance of rubber product, also can be used in medicine, ceramic, plastics, fibre and coating industry, etc. at present, the domestic and foreign active zinc oxide preparation method mainly includes physical method and chemical ammonia compounding method, in which the physical method is mainly zinc sulfate sintering oxidation method, and its energy consumption is high, and the prepared zinc oxide has low purity, and the chemical method uses more ammonium salt-zinc carbonate precursor method, and at present the main problems of said method are that its reaction temperature is high, energy consumption is high, ammonia pollution is high, treatment cost is high, and at the same time zinc yield is not high. The microwave method has few researches at present, uniform microwave heating, easy power control and certain potential in the aspect of new material preparation, and needs to be developed.
Disclosure of Invention
Based on the method, the preparation process of the active zinc oxide provided by the invention promotes the generation of the intermediate small-particle-size basic zinc carbonate through the combined control of microwaves and ultrasound, and the finally prepared zinc oxide has the advantages of small particle size, high purity, good uniformity and large specific surface area.
The technical scheme of the invention is as follows:
the preparation process of the active zinc oxide is characterized by comprising the following steps of:
(1) Collecting zinc-containing smoke dust: putting zinc-containing smoke dust into a solution containing ammonium carbonate, ammonia water and an organic solvent, performing ultrasonic leaching, and centrifuging to remove impurities to obtain a supernatant which is a zinc-ammonia solution;
(2) Microwave heating: placing the zinc ammonia solution into a container, adding a reaction promoter, carrying out a reaction for 2-4 hours by combining a microwave heating method and an ultrasonic method, filtering, collecting a precipitate, obtaining basic zinc carbonate, and drying;
(3) Pretreatment of basic zinc carbonate: washing the dried basic zinc carbonate with 0.2-0.4mol/L ammonia water, and washing with tetrachloromethane for 2-6 times;
(4) And (3) drying: drying the basic zinc carbonate obtained after the treatment in the step 3 at the temperature of 90-100 ℃;
(5) Calcining: calcining the obtained basic zinc carbonate in a horse boiling furnace for 1-2h at high temperature to obtain the active zinc oxide.
Further, in the preparation process of the active zinc oxide, the zinc content of the zinc ammonia solution in the step 1 is controlled to be 15-30g/L.
Further, in the preparation process of the active zinc oxide, the organic solvent in the step 1 is triethanolamine.
Further, in the above preparation process of active zinc oxide, in the step 1, the power of ultrasound is 450-800W.
Further, in the above preparation process of active zinc oxide, in the step 2, the frequency of the microwave is 2100-2500MHz; the power of the ultrasonic wave is 600-1200W.
Further, in the preparation process of the active zinc oxide, the reaction promoter in the step 2 is methyl benzoate.
Further, in the preparation process of the active zinc oxide, the high temperature in the step 5 is 400-600 ℃.
Further, the preparation process of the active zinc oxide comprises the following steps:
(1) Collecting zinc-containing smoke dust: putting zinc-containing smoke dust into a solution containing ammonium carbonate, ammonia water and an organic solvent, performing ultrasonic leaching, and centrifuging to remove impurities to obtain a supernatant which is a zinc-ammonia solution;
(2) Microwave heating: placing the zinc-ammonia solution into a container, adding a reaction promoter, carrying out a reaction for 34 hours by combining microwave heating and an ultrasonic method, filtering and collecting a precipitate to obtain basic zinc carbonate, and drying;
(3) Pretreatment of basic zinc carbonate: washing the dried basic zinc carbonate with 0.3mol/L ammonia water, and washing with tetrachloromethane for 4 times;
(4) And (3) drying: drying the basic zinc carbonate obtained after the treatment in the step 3 at the temperature of 95 ℃;
(5) Calcining: calcining the obtained basic zinc carbonate in a horse boiling furnace for 1.5h at high temperature to obtain the active zinc oxide.
Compared with the prior art, the invention has the beneficial effects that:
the invention utilizes the microwave and ultrasonic combined radiation method to control the particle size and the dispersity of the intermediate basic zinc carbonate by adjusting the microwave frequency and the ultrasonic power, and compared with the conventional heating method, the method is more uniform and thorough, thereby preparing small-particle-size and high-purity zinc oxide according to the basic zinc carbonate with small particle size and reaching the national first-class standard.
Detailed Description
A preparation process of active zinc oxide comprises the following steps:
(1) Collecting zinc-containing smoke dust: putting zinc-containing smoke dust into a solution containing ammonium carbonate, ammonia water and an organic solvent, performing ultrasonic leaching, and centrifuging to remove impurities to obtain a supernatant which is a zinc-ammonia solution; the zinc content of the zinc ammonia solution is controlled to be 15-30g/L; the organic solvent is preferably triethanolamine; the ultrasonic power is 450-800W;
(2) Microwave heating: placing the zinc ammonia solution into a container, adding a reaction promoter, carrying out a reaction for 2-4 hours by combining a microwave heating method and an ultrasonic method, filtering, collecting a precipitate, obtaining basic zinc carbonate, and drying; the frequency of the microwaves is 2100-2500MHz; the power of the ultrasonic wave is 600-1200W; the reaction promoter is methyl benzoate;
(3) Pretreatment of basic zinc carbonate: washing the dried basic zinc carbonate with 0.2-0.4mol/L ammonia water, and washing with tetrachloromethane for 2-6 times;
(4) And (3) drying: drying the basic zinc carbonate obtained after the treatment in the step 3 at the temperature of 90-100 ℃;
(5) Calcining: calcining the obtained basic zinc carbonate in a horse boiling furnace for 1-2h at high temperature to obtain the active zinc oxide; the high temperature is 400-600 ℃.
The technical scheme of the invention will be further described in detail below with reference to specific embodiments. The following examples are illustrative only and are not to be construed as limiting the scope of the invention. All techniques implemented based on the above description of the invention are intended to be included within the scope of the invention.
Unless otherwise indicated, the starting materials and reagents used in the following examples were either commercially available or may be prepared by known methods.
Example 1
A preparation process of active zinc oxide comprises the following steps:
(1) Collecting zinc-containing smoke dust: putting zinc-containing smoke dust into a solution containing ammonium carbonate, ammonia water and an organic solvent, performing ultrasonic leaching, and centrifuging to remove impurities to obtain a supernatant which is a zinc-ammonia solution; the zinc content of the zinc ammonia solution is controlled to be 15g/L; the organic solvent is triethanolamine; the ultrasonic power is 450W;
(2) Microwave heating: putting the zinc-ammonia solution into a container, adding a reaction promoter, carrying out a reaction for 2 hours by combining microwave heating and an ultrasonic method, filtering and collecting a precipitate to obtain basic zinc carbonate, and drying; the frequency of the microwaves is 2500MHz; the power of the ultrasonic wave is 1200W; the reaction promoter is methyl benzoate;
(3) Pretreatment of basic zinc carbonate: washing the dried basic zinc carbonate with 0.2mol/L ammonia water, and washing with tetrachloromethane for 2 times;
(4) And (3) drying: drying the basic zinc carbonate obtained after the treatment in the step 3 at 90 ℃;
(5) Calcining: calcining the obtained basic zinc carbonate in a horse boiling furnace for 1h at high temperature to obtain the active zinc oxide; the high temperature was 600 ℃.
Example 2
A preparation process of active zinc oxide comprises the following steps:
(1) Collecting zinc-containing smoke dust: putting zinc-containing smoke dust into a solution containing ammonium carbonate, ammonia water and an organic solvent, performing ultrasonic leaching, and centrifuging to remove impurities to obtain a supernatant which is a zinc-ammonia solution; the zinc content of the zinc ammonia solution is controlled to be 25g/L; the organic solvent is triethanolamine; the ultrasonic power is 600W;
(2) Microwave heating: putting the zinc-ammonia solution into a container, adding a reaction promoter, carrying out a reaction for 3 hours by combining microwave heating and an ultrasonic method, filtering and collecting a precipitate to obtain basic zinc carbonate, and drying; the frequency of the microwaves is 2300MHz; the power of the ultrasonic wave is 900W; the reaction promoter is methyl benzoate;
(3) Pretreatment of basic zinc carbonate: washing the dried basic zinc carbonate with 0.3mol/L ammonia water, and washing with tetrachloromethane for 4 times;
(4) And (3) drying: drying the basic zinc carbonate obtained after the treatment in the step 3 at the temperature of 95 ℃;
(5) Calcining: calcining the obtained basic zinc carbonate in a horse boiling furnace for 1.5 hours at high temperature to obtain the active zinc oxide; the high temperature is 500 ℃.
Example 3
A preparation process of active zinc oxide comprises the following steps:
(1) Collecting zinc-containing smoke dust: putting zinc-containing smoke dust into a solution containing ammonium carbonate, ammonia water and an organic solvent, performing ultrasonic leaching, and centrifuging to remove impurities to obtain a supernatant which is a zinc-ammonia solution; the zinc content of the zinc ammonia solution is controlled to be 30g/L; the organic solvent is triethanolamine; the ultrasonic power is 800W;
(2) Microwave heating: putting the zinc-ammonia solution into a container, adding a reaction promoter, carrying out a reaction for 4 hours by combining microwave heating and an ultrasonic method, filtering and collecting a precipitate to obtain basic zinc carbonate, and drying; the frequency of the microwaves is 2100MHz; the power of the ultrasonic wave is 600W; the reaction promoter is methyl benzoate;
(3) Pretreatment of basic zinc carbonate: washing the dried basic zinc carbonate with 0.4mol/L ammonia water, and washing with tetrachloromethane for 6 times;
(4) And (3) drying: drying the basic zinc carbonate obtained after the treatment in the step 3 at the temperature of 100 ℃;
(5) Calcining: calcining the obtained basic zinc carbonate in a horse boiling furnace for 2 hours at high temperature to obtain the active zinc oxide; the high temperature is 400 ℃.
Test case
Active zinc oxide was prepared as in examples 1-3 and tested in comparison to commercially available active zinc oxide products. The specific surface areas and the contents of the zinc oxide products prepared in the examples and the comparative examples are detected, and the specific surface area detection method is carried out by referring to national standard (GB/T19587-2004) for measuring the specific surface area of solid substances by a gas adsorption BET method; the detection method of the zinc oxide content is carried out by referring to national standard nano zinc oxide (GB/T19589-2004).
Table 1 comparative test
| Example 1 | Example 2 | Example 3 | Comparative example | |
| Zinc oxide content/% | 98.1 | 99.2 | 97.8 | 96.2 |
| Average particle size/um | 2.7 | 2.1 | 2.9 | 4.1 |
| Specific surface area/m 2 | 47 | 54 | 50 | 48 |
From the data in Table 1, it can be seen that the specific surface area and zinc oxide content of the zinc oxide products prepared according to the present invention are significantly better than those of the comparative examples.
The foregoing description is only of the preferred embodiments of the invention. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (1)
1. The preparation process of the active zinc oxide is characterized by comprising the following steps of:
(1) Collecting zinc-containing smoke dust: putting zinc-containing smoke dust into a solution containing ammonium carbonate, ammonia water and an organic solvent, performing ultrasonic leaching, and centrifuging to remove impurities to obtain a supernatant which is a zinc-ammonia solution;
(2) Microwave heating: placing the zinc-ammonia solution into a container, adding a reaction promoter, carrying out a reaction for 34 hours by combining microwave heating and an ultrasonic method, filtering and collecting a precipitate to obtain basic zinc carbonate, and drying;
(3) Pretreatment of basic zinc carbonate: washing the dried basic zinc carbonate with 0.3mol/L ammonia water, and washing with tetrachloromethane for 4 times;
(4) And (3) drying: drying the basic zinc carbonate obtained after the treatment in the step 3 at the temperature of 95 ℃;
(5) Calcining: calcining the obtained basic zinc carbonate in a muffle furnace for 1.5h at high temperature to obtain the active zinc oxide;
the zinc content of the zinc ammonia solution in the step (1) is controlled to be 15-30g/L;
the organic solvent in the step (1) is triethanolamine;
in the step (1), the power of the ultrasonic wave is 450-800W;
in the step (2), the frequency of the microwaves is 2100-2500MHz; the power of the ultrasonic wave is 600-1200W;
the reaction promoter in the step (2) is methyl benzoate;
the high temperature in the step (5) is 400-600 ℃.
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Citations (5)
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|---|---|---|---|---|
| CN1616354A (en) * | 2003-11-14 | 2005-05-18 | 湘潭大学 | Uniformly coordinating precipitation method for preparing nano zinc oxide |
| CN103145176A (en) * | 2013-02-04 | 2013-06-12 | 唐山海港合缘锌业有限公司 | High-activity empty frame zinc oxide production method by means of industrial zinciferous smoke dust |
| CN108002423A (en) * | 2017-12-19 | 2018-05-08 | 云南锡业职业技术学院 | The method that a kind of ultrasonic wave and microwave cooperating prepare nano zine oxide |
| CN108328642A (en) * | 2018-02-01 | 2018-07-27 | 昆明理工大学 | A method of non-evaporating hair prepares basic zinc carbonate from zinc ammonia solution |
| CN108862372A (en) * | 2018-07-24 | 2018-11-23 | 重庆东群科技有限公司 | A method of nano zine oxide and compound of calcium carbonate are produced using containing zinc ore crude |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9528170B2 (en) * | 2012-09-25 | 2016-12-27 | Sichuan Xinhong Technology Co., Ltd | Method for producing a high-purity nanometer zinc oxide from steel plant smoke and dust by ammonia decarburization |
| US10407315B2 (en) * | 2016-04-14 | 2019-09-10 | Seoul Semiconductor Co., Ltd. | Method and/or system for synthesis of zinc oxide (ZnO) |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1616354A (en) * | 2003-11-14 | 2005-05-18 | 湘潭大学 | Uniformly coordinating precipitation method for preparing nano zinc oxide |
| CN103145176A (en) * | 2013-02-04 | 2013-06-12 | 唐山海港合缘锌业有限公司 | High-activity empty frame zinc oxide production method by means of industrial zinciferous smoke dust |
| CN108002423A (en) * | 2017-12-19 | 2018-05-08 | 云南锡业职业技术学院 | The method that a kind of ultrasonic wave and microwave cooperating prepare nano zine oxide |
| CN108328642A (en) * | 2018-02-01 | 2018-07-27 | 昆明理工大学 | A method of non-evaporating hair prepares basic zinc carbonate from zinc ammonia solution |
| CN108862372A (en) * | 2018-07-24 | 2018-11-23 | 重庆东群科技有限公司 | A method of nano zine oxide and compound of calcium carbonate are produced using containing zinc ore crude |
Non-Patent Citations (2)
| Title |
|---|
| 精细化工.微波加热制备纳米ZnO粉体及其表征.《精细化工》.2003,第20卷(第20期),265-267. * |
| 闫金龙 ; 郭小华 ; 王保安 ; .氨浸取粗氧化锌粉中锌的工艺研究.广州化学.2012,(04),534-537. * |
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